Particle Metrology Research Articles

Particle metrology and classification instrumentation based on dual-wavelength illumination and modulated polarization detection

Particle metrology and classification instrumentation based on dual-wavelength illumination and modulated polarization detection

Particle Metrology Approach to Understanding How Storage Conditions Affect Long-Term Liposome Stability.

Lipid nanoparticles are a generic type of nanomaterial with broad applicability in medicine as drug delivery vehicles. Liposomes are a subtype of lipid nanoparticles and, as a therapeutic platform, can be loaded with a genetic material or pharmaceutical agents for use as drug treatments. An open question for these types of lipid nanoparticles is what factor(s) affect the long-term stability of the particles. The stability of the particle is of great interest to understand and predict the effective shelf-life and storage requirements. In this report, we detail a one-year study of liposome stability as a function of lipid composition, buffer composition/pH, and storage temperature. This was done in aqueous solution without freezing. The effect of lipid composition is shown to be a critical factor when evaluating stability of the measured particle size and number concentration. Other factors (i.e., storage temperature and buffer pH/composition) were shown to be less critical but still have some effect. The stability of these particles informs formulation and optimal storage requirements and assists with future developmental planning of a NIST liposome-based reference material. This work also highlights the complex nature of long-term soft particle storage in biopharmaceutical applications.

Particle tracking and identification using on-chip holographic imaging with inertial separation

Rapid and accurate monitoring and identification of micro-sized particles are of utmost importance in various industrial fields. Here, we present an on-chip microscopy holography platform with an inertial impactor for particle metrology and classification. In particular, the particles are first sampled and classified via an inertial impactor according to their inertia. By interrogating the particle location and size using digital in-line holography imaging techniques with calibrated models, we, for the first time, classify particles with different inertia and estimate the particle mass densities. We then develop an IOS-based App interface for wirelessly controlling of the CMOS imager and sample image reconstruction process. The imaging platform proposed in work have prominent advantages including compact in size, robust and efficient in reconstruction algorithm, high throughput characterization capability. Additionally, it can operate remotely via smartphone and a customized App interface, which is especially relevant for industrial application where on-site/remote metrology and identification of particles is required.

Statistically Representative Metrology of Nanoparticles via Unsupervised Machine Learning of TEM Images.

The morphology of nanoparticles governs their properties for a range of important applications. Thus, the ability to statistically correlate this key particle performance parameter is paramount in achieving accurate control of nanoparticle properties. Among several effective techniques for morphological characterization of nanoparticles, transmission electron microscopy (TEM) can provide a direct, accurate characterization of the details of nanoparticle structures and morphology at atomic resolution. However, manually analyzing a large number of TEM images is laborious. In this work, we demonstrate an efficient, robust and highly automated unsupervised machine learning method for the metrology of nanoparticle systems based on TEM images. Our method not only can achieve statistically significant analysis, but it is also robust against variable image quality, imaging modalities, and particle dispersions. The ability to efficiently gain statistically significant particle metrology is critical in advancing precise particle synthesis and accurate property control.

Multiple Technique Characterization of the Physical and Chemical Properties of Silica Abrasives Used in Chemical-Mechanical Planarization

The performance of chemical-mechanical planarization (CMP) slurries in the commercial fabrication of integrated circuits depends critically on the physical and chemical properties of abrasive particles used in CMP slurries. A host of analytical methods are used for characterizing the properties of CMP abrasive particles including spectroscopic,1,2 sedimentation,3 viscometric4 and fractionation5 techniques. One particular method, fluorescence correlation spectroscopy (FCS),1 has demonstrated significant versatility in this application due to its ability to simultaneously analyze the particle size distribution and the surface chemistry of abrasive particles in aqueous mixture containing small molecule CMP additives. The need for further characterization of these properties, especially the surface chemistry, is the product of the increasing use of nano-abrasives with reduced hydrodynamic diameters (< 20 nm) in CMP slurries in order to minimize surface defect creation during CMP processes. Incorporation of nano-abrasives in CMP slurries will promote surface chemistry-driven CMP additive adsorption on abrasive particles due to the increase in the total particle surface area as the hydrodynamic diameters of nano-abrasives decrease. The use of FCS in conjunction with the application of complementary techniques, such as dynamic light scattering and fluorescence lifetime analysis, is described in the presentation for the comprehensive characterization of the physical and chemical properties of representative silica abrasives used in CMP slurries.1. Jacobson, L.M.; Turner, D.K.; Wayman, A.; Rawat, A.; Carver, C.T..; Moinpour, M.; Remsen, E.E. “Characterization of Particle Size and Surface Adsorption for SiO2 Abrasives Used in Chemical Mechanical Planarization via Fluorescence Correlation Spectroscopy”, ECS J. Solid State Sci. Tech. 2015, 4, P5053-P5057.2. Marsh, J.L.; Wayman, A.E.; Smiddy, N.M.; Campbell, D.J.; Parker, J.C.; Bosma, W.B.; Remsen, E.E. “Infrared Spectroscopic Analysis of the Adsorption of Pyridine Carboxylic Acids on Colloidal Ceria”, Langmuir 2017, 33 , 13224-13233.3. Kamiti, M.; Boldridge, D.; Ndoping, L.M.; Remsen, E.E. “Simultaneous Absolute Determination of Particle Size and Effective Density of sub-Micron Colloids by Disc Centrifuge Photosedimentometry”, Anal. Chem. 2012, 84, 10526−10530. 4. Boldridge, D.; Kamiti, M.; Remsen, E.E. “Avoiding the Spherical Particle Assumption: Fractal Particle Density, Size and Structure Characterization through Combined Sedimentation and Viscometry Measurements”, Anal. Chem. 2020, 92, 15034-15041.5. Williams, S.K.R.; Park, I.; Remsen, E.E.; Moinpour, M. “New Particle Metrology for CMP Slurries”, Mater. Res. Soc. Symp. Proc. 2007, 991, 249-251.

Single Particle Inductively Coupled Plasma Mass Spectrometry Study of Ceria Nanoparticle Size Distribution from 300mm Wafer Oxide CMP with Microreplicated Pads

This work describes the use of Single Particle Inductively Coupled Plasma Mass Spectrometry (spICP-MS) to measure ceria particle number concentrations and compare changes in size distributions to silicon dioxide wafer removal rates from different chemical mechanical planarization (CMP) processes. Particle number concentrations were measured for the 21 to 559 nm size range at 1nm size resolution. Changes in the ceria particle size distribution after CMP included a decrease in large (>130 nm) particles, an increase in small (<40 nm) particles, an increase in the total number of particles, and a decrease in median particle size. The decrease in median size was as high as 7% and influenced by slurry flow rate, wafer pressure and pad type. A novel microreplicated CMP pad was used which requires no pad conditioning to ensure consistent pad surface features, and the effect of different pad types on removal rate and particle size was isolated. A decrease in the median particle size correlated with higher silicon dioxide removal rates (R2=0.96) for a series of pad types with unique combinations of chemistry and surface features. This new combination of nano particle metrology and control of pad surface features is an improved tool set for modeling advanced CMP processes.

Single Particle Inductively Coupled Plasma Mass Spectrometry Study of Ceria Nanoparticle Size Distribution from Oxide CMP with Microreplicated Pads

This work describes the use of Single Particle Inductively Coupled Plasma Mass Spectrometry (spICP-MS) to measure ceria particle number concentrations and compare changes in size distributions to silicon dioxide wafer removal rates from different chemical mechanical planarization (CMP) processes. Particle number concentrations were measured for the 21 to 559 nm size range at 1 nm size resolution. Changes in the ceria particle size distribution after CMP included a decrease in large (>130 nm) particles, an increase in small (<40 nm) particles, an increase in the total number of particles, and a decrease in median particle size. The decrease in median size was as high as 7% and influenced by flow rate, pressure and pad type. A novel microreplicated CMP pad was used which requires no pad conditioning to ensure consistent pad surface features, and the effect of different pad types on removal rate and particle size was isolated. A decrease in the median particle size correlated with higher silicon dioxide removal rates (R2 = 0.96) for a series of pad types with unique combinations of chemistry and surface features. This new combination of nano particle metrology and control of pad surface features is an innovative tool set for modeling advanced CMP processes.

A Concept for Three-Dimensional Particle Metrology Based on Scanning Electron Microscopy and Structure-from-Motion Photogrammetry.

Scanning electron microscopy (SEM) has been frequently used for size and shape measurements of particles. SEM images offer two-dimensional (2D) information about a particle’s lateral dimensions. Unfortunately, information about the particle’s three-dimensional (3D) size and shape remains unavailable. To resolve this issue, I propose a new concept in SEM: 3D particle metrology obtained by applying structure-from-motion (SfM) algorithms to multiple rotational SEM images of particles deposited onto a cylindrical substrate to generate a 3D model from which size and shape information can be extracted. Particles can have any size that is suitable for SEM imaging. SEM images of the sample can be acquired from 0° to 360° using a rotational-tip SEM substage. Here, I will discuss the concept and, for clarity, illustrate it with aquarium gravel particles that are glued onto a craft roll and imaged optically before generating the 3D model of that handmade craft. Future work will include the experimental SEM realization, as well as further development of the SfM algorithms. In my view, this proposed concept may become an integral part of SEM-based particle metrology.

Calibration of optical particle counters: first comprehensive inter-comparison for particle sizes up to 5 µm and number concentrations up to 2 cm−3

We report on an inter-laboratory comparison for the calibration of light-scattering optical particle counters measuring the number concentration of airborne particles in the size range 300 nm–5 µm. This comparison, registered as EURAMET pilot study Nr. 1453, is an important first step towards internationally recognized SI traceability in the measurement of low particle number concentrations encountered in clean-room facilities. The participating particle metrology laboratories of NMIJ (Japan), DFM (Denmark) and METAS (Switzerland) each provided a portable optical particle counter as a transfer standard to be circulated amongst the partners. The comparison covered particle number concentrations up to about 2 cm−3. The individual measurements for the transfer standards at each laboratory are in good agreement with the reference value, typically within 7%, which supports the applied national primary methods of measurement.

On-the-fly particle metrology in hollow-core photonic crystal fibre.

Efficient monitoring of airborne particulate matter (PM), especially particles with aerodynamic diameter less than 2.5 µm (PM2.5), is crucial for improving public health. Reliable information on the concentration, size distribution and chemical characteristics of PMs is key to evaluating air pollution and identifying its sources. Standard methods for PM2.5 characterization require sample collection from the atmosphere and post-analysis using sophisticated equipment in a laboratory environment, and are normally very time-consuming. Although optical methods based on analysis of scattering of free-space laser beams or evanescent fields are in principle suitable for real-time particle counting and sizing, lack of knowledge of the refractive index in these methods not only leads to inevitable sizing ambiguity but also prevents identification of the particle material. In the case of evanescent wave detection, the system lifetime is strongly limited by adhesion of particles to the surfaces. Here we report a novel technique for airborne particle metrology based on hollow-core photonic crystal fibre. It offers in situ particle counting, sizing and refractive index measurement with effectively unlimited device lifetime, and relies on optical forces that automatically capture airborne particles in front of the hollow core and propel them into the fibre. The resulting transmission drop, together with the time-of-flight of the particles passing through the fibre, provide unambiguous mapping of particle size and refractive index with high accuracy. The technique offers unique advantages over currently available real-time particle metrology systems, and can be directly applied to monitoring air pollution in the open atmosphere as well as precise particle characterization in a local environment such as a closed room or a reaction vessel.

Infrared Technologies for Defence Systems

&lt;p&gt; Infrared technology has seen phenomenal growth since its inception during World War II. Defence applications have been the main driver of infrared technology development all over the world. Infrared systems have been mainly developed for night vision, all weather surveillance, search and tracking and missile seeker applications. Ever demanding defence system requirements have facilitated considerable investment. Research has been mainly directed towards the product development. Medical applications such as thermographs, transportation applications such as enhanced vision systems for airplanes, helicopters, sea vehicles, and automobiles, law enforcement applications in drug prevention and criminal tracking, managing forest fires and environmental monitoring are some of the spin-offs. Infrared technology has proven to be a force multiplier in war as well as low intensity conflict situation. Intelligent vision sensor development covering visible-infrared spectrum for automated surveillance, change detection, 3D machine vision systems, dynamic particle metrology, missile and ballistic testing/imaging, faster, more precise and more manoeuvrable robotic applications will drive the future research.&lt;/p&gt;

Backscattering measurements of micron-sized spherical particles.

An apparatus was designed and assembled to measure scattered light in the range of 180°±6° where enhanced backscattering, the cause of a glory, occurs. The apparatus was calibrated and tested using Fraunhofer circular aperture diffraction, angle of incidence correction, and a diffuse reflector. Theory indicates that backscattering is strongly dependent on particle size, refractive index, and shape. Experimental measurements from polystyrene latex spheres of two sizes and water droplets showed good agreement with Mie theory, but also indicated the extreme sensitivity of the backscattering to particle parameters. The results presented should have use in the fields of particle scattering, particle metrology, and LIDAR.

Particle number density gradient samples for nanoparticle metrology with atomic force microscopy

Nanoparticle metrology with atomic force microscope (AFM) aims to determine an average particle size from measurements of individual nanoparticles derived by image analysis. This constrains the statistical relevance of the measurement due to the limited number of particles which can be practically imaged and analyzed. Consequently, the number density of particles on samples prepared for particle measurement is an important parameter of sample preparation. A number density that is too low makes it difficult to obtain sufficient measurement statistics, whereas a number density that is too high can result in particle agglomeration on the substrate and limit the area of uncovered substrate that is required to obtain a reliable reference for measuring the particle height. We present imaging and measurement results of a particle number density gradient of 16 nm gold nanoparticles deposited using a gradual immersion process. Results demonstrate how samples with particle number density gradients can facilitate identification of an area on a sample with optimal particle number density for AFM particle metrology and thereby improve measurement efficiency and reliability.

Three-dimensional particle imaging by defocusing method with an annular aperture

We propose an annular-aperture-based defocusing technique for three-dimensional (3D) particle metrology from a single camera view. This simple configuration has high optical efficiency and the ability to deal with overlapped defocused images. Initial results show that an uncertainty in depth of 23 microm can be achieved over a range of 10 mm for macroscopic systems. This method can also be applied in microscopy for the measurement of fluorescently doped microparticles, thus providing a promising solution for 3D flow metrology at both macroscales and microscales.

Particle Metrology in CMP Slurries - Potential and Limitations of Relevant Measuring Methods

ABSTRACTThe design of nanostructured materials like CMP slurries on an industrial scale requires the control of disperse systems of nanoparticles as well as of single isolated "bad" particles . It is well known that slurry abnormalities resulting from large abrasive particles and abrasive particles agglomeration can cause defects on wafer surfaces during CMP.Particle-particle interactions generate secondary nanometer structures, clusters or agglomerates, which can dominate the relevant properties of the bulk material. Size and structure of these particle agglomerates/structures are the result of a dynamic equilibrium between agglomeration and desagglomeration. There is still a lack of understanding of these secondary soft nano- up to micro- particles because no adequate characterization methods are established.Dilution and other preparation treatment to enable analysis by laboratory methods like TEM or AFM will distort the interparticle forces and will generate artifacts. Hence characterization methods are under investigation which can tolerate a high number of particles in the sensing zone. These high concentration methods often deliver ambiguous results. Consequently different physical principles have to be combined to get unambiguous information on the disperse state.Performance characteristics of ultrasonic spectroscopy, photon correlation spectroscopy, analytical photo-centrifugation method combined with the high spatial resolution as well as special single particle optical counters are discussed on examples.

Three-dimensional particle imaging by wavefront sensing

We present two methods for three-dimensional particle metrology from a single two-dimensional view. The techniques are based on wavefront sensing where the three-dimensional location of a particle is encoded into a single image plane. The first technique is based on multiplanar imaging, and the second produces three-dimensional location information via anamorphic distortion of the recorded images. Preliminary results show that an uncertainty of 8 microm in depth can be obtained for low-particle density over a thin plane, and an uncertainty of 30 microm for higher particle density over a 10 mm deep volume.

Neutrino mass and low-temperature calorimetry

We describe how the problem of measuring the neutrino mass led us to the development of low-temperature calorimetry. The search for a “17-keV neutrino” concluded with a negative result, but a wide range of applications are now carried on by us and other groups in the fields of x-ray astronomy, recoil measurements of dark matter particles, high precision particle spectrometry, specific heat determinations, neutron detection, and rare decay studies. The masses of the bolometers (calorimeters) extend from 1 mg to 1 kg, nearly as large as for quantum detectors. By lowering the temperature into the 10- 20-mK range, calorimetry is on its way to substantially surpassing the high precision of particle metrology obtainable with the quantum detectors. Calorimeter developments and perspectives are discussed.

LIQUID‐BORNE PARTICLE METROLOGY

The SciencesVolume 8, Issue 4 p. 29-31 LIQUID-BORNE PARTICLE METROLOGY First published: April 1968 https://doi.org/10.1002/j.2326-1951.1968.tb00357.xAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat Volume8, Issue4April 1968Pages 29-31 RelatedInformation